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class="spacer" data-v-cb998dce></div><!--[--><!--]--><!----><!--[--><!--]--><!--[--><!--]--></div></div></div></div><div class="content" data-v-e6f2a212><div class="content-container" data-v-e6f2a212><!--[--><!--]--><main class="main" data-v-e6f2a212><div style="position:relative;" class="vp-doc _sop_sops_%E5%86%B7%E6%B5%B4" data-v-e6f2a212><div><h1 id="冷浴-cooling-baths" tabindex="-1">冷浴 Cooling Baths <a class="header-anchor" href="#冷浴-cooling-baths" aria-label="Permalink to &quot;冷浴 Cooling Baths&quot;">​</a></h1><ul><li>贡献者：zjxxx；整理：陈心怡</li></ul><p>Often it is necessary to use cooling baths to chill a reaction below 0 ºC (Table 1.4). The low temperature could be important for a variety of reasons, including stereoselectivity dependence, decomposition of reagents, and decomposition of products. Thus, a simple and inexpensive method for maintaining the reaction is with a cooling bath. A cooling bath can be produced by creating a slush with solvent and ice, solid CO<sub>2</sub> (dry ice), or liquid nitrogen in a Dewar flask. To maintain the temperature, additional amounts of ice, dry ice, or liquid nitrogen must added. However, an internal thermometer should be used to determine the actual temperature of the reaction mixture.</p><p>通常需要使用冷却浴来将反应冷却到0℃以下（表1.4）。这个低温环境有时很重要，原因有很多，包括立体选择性依赖、试剂的分解和产物的分解等。就此而言，维持反应的一种简单廉价的方式就是使用冷却浴。冷却浴的环境可以通过溶剂和冰制成的冷却剂、固体二氧化碳（干冰）或者真空瓶中的液氮营造。为了保持冷却浴的温度，必须额外地添加大量的冰、干冰或液氮。但是对于反应混合物的实际温度，应使用置于内部的温度计确定。</p><p>参考资料Reference: Phillips, A. M.; Hume, D. N. J. Chem. Edu. 1968, 54, 664; Armarego, W. L. F.; Perrin, D. D. Purifification of Laboratory Chemicals; 4th ed.; Butterworth Heineman: Oxford, 1996; p. 36</p><h2 id="冷浴-cooling-baths-1" tabindex="-1">冷浴 Cooling Baths <a class="header-anchor" href="#冷浴-cooling-baths-1" aria-label="Permalink to &quot;冷浴 Cooling Baths&quot;">​</a></h2><p>表1.4 冷浴</p><table tabindex="0"><thead><tr><th style="text-align:center;">混合物</th><th style="text-align:center;">温度（℃）</th></tr></thead><tbody><tr><td style="text-align:center;">碎冰</td><td style="text-align:center;">0</td></tr><tr><td style="text-align:center;">冰/氯化钠</td><td style="text-align:center;">-5 到-20</td></tr><tr><td style="text-align:center;">乙二醇/CO₂(s)</td><td style="text-align:center;">-11</td></tr><tr><td style="text-align:center;">四氯化碳/CO₂(s)</td><td style="text-align:center;">-23</td></tr><tr><td style="text-align:center;">庚-3-酮/CO₂(s)</td><td style="text-align:center;">-38</td></tr><tr><td style="text-align:center;">乙腈/CO₂(s)</td><td style="text-align:center;">-41</td></tr><tr><td style="text-align:center;">氯仿/CO₂(s)</td><td style="text-align:center;">-61</td></tr><tr><td style="text-align:center;">乙醇/CO₂(s)</td><td style="text-align:center;">-72</td></tr><tr><td style="text-align:center;">丙酮/CO₂(s)</td><td style="text-align:center;">-78</td></tr><tr><td style="text-align:center;">乙酸乙酯/N₂(1)</td><td style="text-align:center;">-84</td></tr><tr><td style="text-align:center;">甲醇/N₂(1)</td><td style="text-align:center;">-98</td></tr><tr><td style="text-align:center;">乙醇/N₂(1)</td><td style="text-align:center;">-116</td></tr><tr><td style="text-align:center;">戊烷/N₂(1)</td><td style="text-align:center;">-131</td></tr></tbody></table><h2 id="常见的市售格氏试剂-common-commercially-available-reagents" tabindex="-1">常见的市售格氏试剂 Common commercially available reagents <a class="header-anchor" href="#常见的市售格氏试剂-common-commercially-available-reagents" aria-label="Permalink to &quot;常见的市售格氏试剂 Common commercially available reagents&quot;">​</a></h2><p>表1.5 常见的市售格氏试剂</p><table tabindex="0"><thead><tr><th style="text-align:center;">有机镁试剂</th><th style="text-align:center;">溶剂（M浓度）</th></tr></thead><tbody><tr><td style="text-align:center;">甲基氯化镁</td><td style="text-align:center;">THF(3.0)</td></tr><tr><td style="text-align:center;">甲基溴化镁</td><td style="text-align:center;">丁基醚（1.0）、乙醚（3.0）、PhMe/THF(75/25,1.4)</td></tr><tr><td style="text-align:center;">甲基碘化镁</td><td style="text-align:center;">乙醚（1.0）</td></tr><tr><td style="text-align:center;">乙基溴化镁</td><td style="text-align:center;">TBME（1.0）、乙醚（3.0）、THF（1.0）</td></tr><tr><td style="text-align:center;">丙基氯化镁</td><td style="text-align:center;">乙醚（2.0）</td></tr><tr><td style="text-align:center;">异丙基氯化镁</td><td style="text-align:center;">丁基二甘醇（1.4）、乙醚（2.0）、THF(2.0)</td></tr><tr><td style="text-align:center;">叔丁基氯化镁</td><td style="text-align:center;">乙醚（2.0）、THF(1.0)</td></tr><tr><td style="text-align:center;">乙烯基氯化镁</td><td style="text-align:center;">THF(1.0,1.6)</td></tr><tr><td style="text-align:center;">烯丙基溴化镁</td><td style="text-align:center;">乙醚（1.0）</td></tr><tr><td style="text-align:center;">烯丙基氯化镁</td><td style="text-align:center;">THF(2.0)</td></tr><tr><td style="text-align:center;">苯基溴化镁</td><td style="text-align:center;">乙醚（3.0）、THF(1.0)</td></tr><tr><td style="text-align:center;">苯基氯化镁</td><td style="text-align:center;">THF(2.0)</td></tr></tbody></table><p>TBME：丁基甲基醚；THF：四氢呋喃</p><p>参考资料：Sigma-Aldrich. See Sigma-Aldrich ChemFiles 2002, Vol. 2, No.5, for more organomagnesium reagents.</p></div></div></main><footer class="VPDocFooter" data-v-e6f2a212 data-v-1bcd8184><!--[--><!--]--><div class="edit-info" data-v-1bcd8184><!----><div class="last-updated" data-v-1bcd8184><p class="VPLastUpdated" data-v-1bcd8184 data-v-1bb0c8a8>最后编辑: <time datetime="2024-12-03T06:54:35.000Z" data-v-1bb0c8a8></time></p></div></div><!----></footer><!--[--><!--]--></div></div></div><!--[--><!--]--></div></div><footer class="VPFooter" data-v-d8b57b2d data-v-566314d4><div class="container" data-v-566314d4><p class="message" data-v-566314d4>CPU-SOP | 中国药科大学实验标准操作规程(SOP)计划</p><p class="copyright" data-v-566314d4>京ICP备2020036654号-9</p></div></footer><!--[--><!--]--></div></div>
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